Comparative Methodology for Isolation of Flavonoid Glycosides from Clusia criuva Cambess

The family Guttiferae belongs to the superorder Theiflorae, order Theales and according to Dahlgren's system of classification, it is equivalent to Hypericaceae (=Clusiaceae) [1]. This family consists of 49 genera encompassing over 1000 species of wide distribution in the tropics as shrubs and trees [2]. Plants of the genus Clusia have been used in folk medicine for the treatment of different kind of illness such as: febrifuge, anti rheumatic, purgative, for stomach problems and, in Brazil, they are very commonly used to heal wounds [3]. The key of any study of material from natural sources is the availability of suitable separation methods for the isolation of pure products [4–6]. Tentatives for separations using chomatography on solid support phases were not very efficients in the fractionation of Clusia criuva Cambess methanolic/ethyl acetate extracts. However, the use of counter-current chromatography, an all liquid technique, showed advantages in comparison with the more traditional liquid-solid separation methods and even with HPLC. In this sense it was possible to isolate flavonoid glycosides from ethyl acetate extract of Clusia criuva, in a very short operation time.     

Oriented antibody immobilization for atrazine determination by a flow-through fluoroimmunosensor

An atrazine flow-through fluoroimmunosensor was developed, based on an oriented antibody covalently bound to Protein-A (Prot-A) immobilized on Controlled Pore Glass (CPG). Atrazine was detected “in-situ” by placing the immobilized antibody in the optical path of the flow cell. Immobilization of 30 μg of polyclonal anti-atrazine antibody on 0.5 g of Prot-A-CPG provided the highest sensitivity. The effect of several solvents on the covalently immobilized antibodies regeneration was evaluated, the optimum conditions being achieved by pumping 5% acetonitrile (pH = 3) at 0.15 mL/min for 100 s. The detection limit of the immunosensor was 0.7 μg/L and the reproducibility was 2% and 4% for 5 μg/L and 40 μg/L, respectively, in the optimum working concentration range (0.7–50 μg/L). This device allowed 12 samples per hour to be analyzed and had a life-time of 200 assays. Simazine and desisopropylatrazine (DIA) were not cross-reactive, desethylatrazine (DEA) has a cross-reactivity of 8% and propazine and prometryn of 44% and 27%, respectively. The immunosensor was applied to the determination of atrazine in tap and ground water samples spiked at the ?10 and 30 μg/L concentration level. Received: 30 April 1999 / Revised: 16 July 1999 / Accepted: 21 July 1999     

The preparation of a certified reference material of polar pesticides in freeze-dried water (CRM 606)

The preparation of a certified reference material of polar pesticides in freeze-dried water is described. The pesticides selected were atrazine, simazine, carbaryl, propanil, linuron, fenamiphos and permethrin which were added to 6000 litres of tap water at 50–80 μg · L^–1 (200–320 μg · L^–1 for permethrin) level in presence of NaCl (2.5 g · L^–1) prior lyophilization. After the freeze-drying process the residue was rehomogenized, filled into amber glass bottles and stored at –20 °C, +4 °C and +20 °C. All pesticides were determined by HPLC/diode array detector, except permethrin which was determined by GC/ECD. The results obtained for atrazine, simazine, carbaryl, propanil, linuron and fenamiphos showed no within- or between-bottle inhomogeneity, however the material was non-homogeneous for permethrin and therefore this was withdrawn from further studies. With respect to the stability for over one year, all pesticides were stable at –20 °C. At +4 °C all pesticides were stable for at least 9 months and at +20 °C the stability was demonstrated only during the first month of storage. The content (mass fractions) of atrazine, simazine, carbaryl, propanil and linuron in freeze-dried water (CRM 606) was certified by an interlaboratory testing and a certification campaign. Received: 7 September 1998 / Revised: 13 November 1998 / Accepted: 21 November 1998     

Rhodium amino complexes [Rh(COD)(Amine)2]PF6 immobilized on poly(4-vinylpyridine) as catalysts in the water gas shift reaction

Catalysts for the water gas shift reaction prepared from Rh(COD)(amine)₂ PF₆ (COD=1,5-cyclooctadiene, amine=4-picoline, 3-picoline, 2-picoline, pyridine, 3,5-lutidine or 2,6-lutidine) immobilized on poly(4-vinylpyridine) in contact with 80% aqueoux 2-ethoxyethanol for 1×10⁻⁴ mol Rh/0.5 g of polymer, P(CO)=0.9 atm at 100 °C, are described. The role of the coordinated amine effect on the catalytic activity was investigated.     

Acid-Catalyzed Liquefaction of Biomasses from Poplar Clones for Short Rotation Coppice Cultivations

Liquefaction of biomass delivers a liquid bio-oil with relevant chemical and energetic applications. In this study we coupled it with short rotation coppice (SRC) intensively managed poplar cultivations aimed at biomass production while safeguarding environmental principles of soil quality and biodiversity. We carried out acid-catalyzed liquefaction, at 160 °C and atmospheric pressure, with eight poplar clones from SRC cultivations. The bio-oil yields were high, ranging between 70.7 and 81.5%. Average gains of bio-oil, by comparison of raw biomasses, in elementary carbon and hydrogen and high heating, were 25.6, 67, and 74%, respectively. Loss of oxygen and O/C ratios averaged 38 and 51%, respectively. Amounts of elementary carbon, oxygen, and hydrogen in bio-oil were 65, 26, and 8.7%, and HHV averaged 30.5 MJkg⁻¹. Correlation analysis showed the interrelation between elementary carbon with HHV in bio-oil or with oxygen loss. Overall, from 55 correlations, 21 significant and high correlations among a set of 11 variables were found. Among the most relevant ones, the percentage of elementary carbon presented five significant correlations with the percentage of O (−0.980), percentage of C gain (0.902), percentage of O loss (0.973), HHV gain (0.917), and O/C loss (0.943). The amount of carbon is directly correlated with the amount of oxygen, conversely, the decrease in oxygen content increases the elementary carbon and hydrogen concentration, which leads to an improvement in HHV. HHV gain showed a strong positive dependence on the percentage of C (0.917) and percentage of C gain (0.943), while the elementary oxygen (−0.885) and its percentage of O loss (0.978) adversely affect the HHV gain. Consequently, the O/C loss (0.970) increases the HHV positively. van Krevelen’s analysis indicated that bio-oils are chemically compatible with liquid fossil fuels. FTIR-ATR evidenced the presence of derivatives of depolymerization of lignin and cellulose in raw biomasses in bio-oil. TGA/DTG confirmed the bio-oil burning aptitude by the high average 53% mass loss of volatiles associated with lowered peaking decomposition temperatures by 100 °C than raw biomasses. Overall, this research shows the potential of bio-oil from liquefaction of SRC biomasses for the contribution of renewable energy and chemical deliverables, and thereby, to a greener global economy.     

Origin of yellow luminescence from reduced pressure grown bulk GaN crystals

Cathodoluminescence (CL) in the scanning electron microscope has been applied to study the luminescence emission of GaN single crystals grown by LPE methods. CL spectra show the presence of near band edge and of yellow emissions. The latter has been found to be mainly related to rows of hillocks formed at the growth steps. The origin of the yellow luminescence is discussed     

Spectrofluorimetric Determination of Methyl Paraben in Pharmaceutical Preparations by Means of its Dansyl Chloride Derivative

 A spectrofluorimetric method for the determination of methyl paraben based on derivatization with the labelling reagent dansyl chloride (DNS-Cl), is presented. The effect of the reaction variables (pH, DNS-Cl concentration, temperature, reaction time) and instrumental parameters, has been examined. A linear calibration graph in the ng/ml range has been established. The limit of detection is 18 ng/ml with relative standard deviation less than 3%. The proposed method has been satisfactorily applied to determination of the paraben in two pharmaceutical preparations. Received May 25, 1999. Revision October 20, 1999.     

Dependence on crystal parameters of the correlation time between signal and idler beams in parametric down conversion calculated in the Wigner representation

The theory of parametric down conversion within the framework of the Wigner representation has been treated recently in a series of papers using the standard model Hamiltonian. Here we take a more fundamental point of view studying the mechanism, inside the crystal, for the production of the signal and idler beams. We begin from the evolution equations for the quantum field operators, pass to the Wigner function and solve the resulting (Maxwell) equations with the use of the Green's function method. We derive the time dependence of the coincidence detection probability as a function of the parameters of the nonlinear crystal (in particular the length) the radius of the pumping beam, and the bandwidth of the filters in front of the detectors. Received 24 January 2000 and Received in final form 24 March 2000     

On-Line Multicomponent Determination of the Flux of Mixtures of Phenols Through a Liquid Membrane in Real Time

 The analysis of mixtures of four phenolic compounds in an on-line system using UV-visible measurements with a fibre optic probe is discussed in this work. The aim of this system is to provide accurate real time concentration profiles in order to monitor the transport of phenols across a solid supported liquid membrane in both the feed and stripping phases. Different calibration models are taking into account the pH of the solution, using experimental designs and the first derivative in combination with different multivariate approaches like multiple linear regression (MLR), inverted least squares (ILS) and partial least squares regression (PLS). The comparison of all these combinations is carried out by means of the predictive residual error sum of squares (PRESS) evaluated from an independent set of spectra. From this comparison it is concluded that a PLS model using first derivative spectra offers the most accurate and robust prediction in the permeation experiments. Additionally, the stability of the model and the figures of merit obtained are also discussed. Received July 22, 1999. Revision October 23, 2000.     

Path-integral formulation of backward and umklapp scattering for one-dimensional spinless fermions

We present a (1+1)-dimensional fermionic quantum field theory with nonlocal couplings between currents. This model describes an ensemble of spinless fermions interacting through forward, backward, and UMKLAPP scattering processes. We express the vacuum-to-vacuum functional in terms of a nontrivial fermionic determinant. Using path-integral methods, we find a bosonic representation for this determinant and an effective action depending on three scalar fields, of which two correspond to the physical collective excitations and one is an auxiliary field, which can be integrated out using an approximation technique. Translated from Teoreticheskaya i Matematicheskaya Fizika, Vol. 118, No. 3, pp. 488–496, March, 1999.